液相色谱-串联质谱法测定蜂产品中吡虫啉及其3种代谢物  

Determination of Imidacloprid and Its Three Metabolites in Honey and Bee Pollen by Liquid ChromatographyTandem Mass Spectrometry

作　　者：梁秀美 王祥云[1,3] 薛晓锋[4] 齐沛沛[1] 刘真真[1] 刘之炜[1] 周莉[1] 王新全[1] 王强[1] LIANG Xiu-Mei;WANG Xiang-Yun;XUE Xiao-Feng;QI Pei-Pei;LIU Zhen-Zhen;LIU Zhi-Wei;ZHOU Li;WANG Xin-Quan;WANG Qiang(State Key Lab Breeding Base for Zhejiang Sustainable Plant Pest Control, Ministry of Agriculture,Key Lab for Pesticide Residue Detection , Institute of Quality and Standard for Agro-products ,Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China;College of Plant Protection, Nanjing Agricultural University, Nanjing 210095, China;College of Science, China Agricultural University, Beijing 100094, China;Institute of Apiculture Research, Chinese Academy of Agricultural Sciences, Beijing 100093 , China)

机构地区：[1]省部共建国家重点实验室培育基地"浙江省植物有害生物防控重点实验室"农业部农药残留检测重点实验室浙江省农业科学院农产品质量标准研究所,杭州310021 [2]南京农业大学植物保护学院,南京210095 [3]中国农业大学理学院,北京100094 [4]中国农业科学院蜜蜂研究所,北京100093

出　　处：《分析化学》2017年第4期553-559,共7页Chinese Journal of Analytical Chemistry

基　　金：浙江省自然基金项目(No.LQ14B070004);特色农产品全产业链安全风险管控项目(No.ZJNY2016001);蜂产品全产业链安全风险管控项目(No.ZJNY2016001-02)资助

摘　　要：建立了蜂蜜和蜂花粉中吡虫啉及其代谢物吡虫啉烯烃、吡虫啉脲、6-氯烟酸的液相色谱-串联质谱(LC-MS/MS)检测方法。在Qu ECh ERS方法基础上,针对目标物化学性质和样品杂质情况,对提取溶液的p H值、提取次数、净化材料等参数进行了优化。最终以5%甲酸-乙腈溶液提取两次,无水Mg SO_4、NaCl盐析分层,提取液经增强型脂类去除材料(EMR)净化,以LC-MS/MS进行测定,基质外标法进行定量分析。结果表明,蜂蜜和蜂花粉中吡虫啉、吡虫啉烯烃、吡虫啉脲、6-氯烟酸的平均加标回收率为86.0%~111.5%,相对标准偏差在1.7%~9.6%之间,检出限分别为0.20、3.50、0.40和14.00μg/kg,定量限分别为0.60、11.64、1.20和45.00μg/kg。本方法分析速度快、灵敏度高、重现性好,适用于蜂蜜和蜂花粉中吡虫啉及其3种代谢物的快速测定。A method was developed for the determination of imidacloprid and its metabolites imidaclopridolefin,imidacloprid urea and6-chloronicotinic acid in honey and bee pollen by liquid chromatography tandemmass spectrometry(LC-MS/MS).On the basis of typical QuEChERS method’the pH and times of extractionsolvent’sorbents were optimized to ensure the extraction efficiency and the purification of extraction.Finally’the method was developed as follows:matrix was extracted with5%formic acid-acetonitrile twice,and theextraction was cleaned with enhanced matrix removal-lipid(E M R),detected with LC-MS/MS and quantifiedwith external matrix standards.The results indicated that the average spiked recoveries of imidacloprid’imidacloprid olefin’imidacloprid urea and6-chloronicotinic acid in honey and pollen samples were86.0%-111.5%with relative standard deviations(RSDs)of1.7%-9.6%’the LODs were0.20,3.50,0.40and14.00滋g^kg,and the LOQs were0.60,11.64,1.20and45.00滋g^kg.The method was rapid and simplewith high sensitivity and good reproducibility,and suitable for the determination of imidacloprid and its threemetabolites residues in honey and bee pollen.

关 键 词：液相色谱-串联质谱 蜂蜜 蜂花粉 吡虫啉 吡虫啉烯烃 吡虫啉脲 6-氯烟酸 增强型脂类去除材料 

分 类 号：S896.8[农业科学—特种经济动物饲养] O657.63[农业科学—畜牧兽医]